Hydrochloric Acid → HCID 86604860、化合物

HRID 1431998ノート

反応式

HRID 1431998 の反応式
[NH2:1][C@H:2]([CH2:6][C:7]#[CH:8])[C:3]([OH:5])=[O:4].C([O-])([O-])=O.[Na+].[Na+].O.[Cl:16][C:17]1[CH:18]=[C:19]([S:24](Cl)(=[O:26])=[O:25])[CH:20]=[CH:21][C:22]=1[Cl:23].Cl.[Na+].[Cl-]>O.O1CCOCC1.CCOC(C)=O>[Cl:16][C:17]1[CH:18]=[C:19]([S:24]([NH:1][C@H:2]([CH2:6][C:7]#[CH:8])[C:3]([OH:5])=[O:4])(=[O:25])=[O:26])[CH:20]=[CH:21][C:22]=1[Cl:23]

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 7383Benzenesulfonyl chloride, 3,4-dichloro-HCID 2735133Sodium Carbonate MonohydrateHCID 6992713propargylglycine, (R)-

生成物 1

HCID 86604860HCID 86604860、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

(R)-2-Aminopent-4-ynoic acid (16.0 g, 141 mmol) and Na2CO3.H2O (36.8 g, 296 mmol) were dissolved in 500 mL H2O and 300 mL p-dioxane. To this solution was added 3,4-dichlorobenzene-1-sulfonyl chloride (33.0 g, 134 mmol) dropwise over 25 min. The solution was stirred at RT for 19 h. The solution was then acidified with 5N HCl to pH 1. EtOAc (400 mL) and sat'd NaCl aq. (200 mL) were added and organic layer was separated. The aqueous phase was extracted with EtOAc (200 mL×2), and the combined EtOAc extracts were washed with brine (400 mL×4) and dried over Na2SO4. The solvent was removed under reduced pressure and dried in vacuo to yield 38.

後処理

  1. additionwere added
  2. customorganic layer was separated
  3. extractionThe aqueous phase was extracted with EtOAc (200 mL×2)
  4. washthe combined EtOAc extracts were washed with brine (400 mL×4)
  5. dry with materialdried over Na2SO4
  6. customThe solvent was removed under reduced pressure
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-f60cbc4a38a746399d55148764b0adea
出典データセット
uspto-grants-2009_11
特許番号
US07612060B2

反応ノート

読み込み中…